Reaktion #736775

Reaktionsgleichung

Diethyl N-(1,4-dioxaspiro[4.5]decen-8-yl)aminomethylenemalonate

Dowtherm

Dowtherm

→

ethyl 4-hydroxy-6-oxo-5,6,7,8-tetrahydroquinoline-3-carboxylate ethylene ketal

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux
2. 2
   Temperaturthe mixture is heated at 250° for 45 minutes
3. 3
   workup.DISTILLATIONThe low boiling distillate is collected in a Dean-Stark trap
4. 4
   Sonstigethe mixture is evaporated to dryness in vacuo
5. 5
   Sonstigethe residue is triturated with Et2O

Vorschrift

Diethyl N-(1,4-dioxaspiro[4.5]decen-8-yl)aminomethylenemalonate (53 g) in 100 ml of Dowtherm is added to 400 ml of Dowtherm at reflux and the mixture is heated at 250° for 45 minutes. The low boiling distillate is collected in a Dean-Stark trap. After cooling to room temperature, the mixture is evaporated to dryness in vacuo, and the residue is triturated with Et2O to give ethyl 4-hydroxy-6-oxo-5,6,7,8-tetrahydroquinoline-3-carboxylate ethylene ketal.

Quelle